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Acetone → Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 2-Chloro-6-fluorobenzene-1-carbothioamide | HCID 7745242 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide | HCID 18347932 | 46.9% |
反応手順
Into a 50 mL three necked round bottom flask equipped with a magnetic stirrer was added 2-chloro-6-fluorobenzthioamide (3.78 g, 20 mmol) and acetone (20 mL). Dropwise was added iodomethane (2.84 g, 1.24 mL, 20 mmol) and the mixture was allowed to stir at room temperature overnight with monitoring via HPCL (60/40 acetonitrile/water). The solids were removed via filtration and washed with small portions of acetone to give methyl 2-chloro-6-fluorobenzthioimidate hydroiodide as a light yellow solid: 3.1 g (46.9% yield): 1H NMR (DMSO-d6) δ7.7 (m, 1H), 7.5 (m, 2H), 2.7 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06329528B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-67d5220cc59c4cfab38fbd25bef74308 |
| 出典メモ | uspto-grants-2001_12 |